加入收藏| 关于我们 您好,欢迎来到济南金日和化工有限公司网站!

全国咨询热线:13386411819
0531-81762771

当前位置:首页>>新闻中心>>公司新闻>>氨基磺酸在合成中应该注意什么?
氨基磺酸在合成中应该注意什么?
来源:http://www.jnjrh.com 日期:2018-12-27 发布人:admin
1.氨基磺酸的生产方法许多,有二氧化硫与羟胺或丙酮肟为质料的羟胺法,亚硫酸或硫酸盐与液氨为质料的氨化法,尿素与氯磺酸为质料的氯磺化法,以发烟硫酸和尿素为质料的发烟硫酸法,尿素、三氧化硫和硫酸为质料的硫酸法和发烟硫酸法(又称液相法)和液氨经气化与三氧化硫在气相条件下反响的气相法等。国内外具有工业意义的工艺为发烟硫酸法以及三氧化硫与氨直接组成的氨化法两种。由尿素与发烟硫酸在40-70下进行磺化生成氨基磺酸粗品,然后加水进行结晶制得氨基磺酸成品。质料耗费定额:尿素2000kg/t、发烟硫酸1500kg/t。
1. There are many production methods of aminosulfonic acid, such as hydroxylamine method with sulfur dioxide and hydroxylamine or acetone oxime as material, ammoniation method with sulfite or sulfate and liquid ammonia as material, chlorosulfonation method with urea and chlorosulfonic acid as material, fuming sulfuric acid method with fuming sulfuric acid and urea as material, sulfuric acid method with urea, sulfur trioxide and sulfuric acid as material and fuming sulfuric acid method (also called liquid method) and liquid method. The gasification of ammonia and the gas phase reaction of sulfur trioxide under gas phase conditions are the same. There are two processes of industrial significance at home and abroad: fuming sulfuric acid process and ammoniation process, which is directly composed of sulfur trioxide and ammonia. Sulfonated urea and fuming sulfuric acid at 40-70 to produce crude sulfamic acid, then added water to crystallize to produce sulfamic acid products. Material consumption quota: urea 2000 kg/t, fuming sulfuric acid 1500kg/t.
2.其组成方法首要有气相法和液相法两种。气相法操作条件严苛,设备原料要求高。副产品多,且氨基酸易粘附在反响器内壁需常常清理。生产成本高。长处是产品纯度高。厂家采用的多为液相法。
2. The gas phase method and the liquid phase method are the main methods of its composition. Gas phase method has strict operating conditions and high requirements for equipment raw materials. There are many by-products, and amino acids are easy to adhere to the inner wall of the reactor and need to be cleaned frequently. The production cost is high. The advantage is that the product is of high purity. Most of the methods used by manufacturers are liquid phase method.
3.将过量的发烟硫酸参加反响釜中,拌和降温至20~40,开始参加按比例混合好的硫酸和尿素。加料完毕后,在20左右拌和8h。再逐步升温至70~90,蒸出三氧化硫,冷却析晶。固液分享后得粗氨基磺酸,用水重结晶,脱水干燥得高纯度精品氨基磺酸。
氨基磺酸
3. Participate excessive fuming sulfuric acid in the reactor, mix and cool down to 20-40, and begin to participate in proportionally mixed sulfuric acid and urea. After filling, mix for about 20 hours and 8 hours. Then the temperature is gradually increased to 70-90, sulfur trioxide is evaporated, and crystallization is cooled. After solid-liquid sharing, crude aminosulfonic acid was obtained, recrystallized with water and dehydrated to obtain high-purity and high-quality aminosulfonic acid.
4.氨基磺酸是强Lewis酸SO3与强Lewis碱NH3的加合物,制取少数纯度要求高的氨基磺酸时,可在彻底无水的条件下,直接用高纯度的SO3与氨反响。若用量较大时可用尿素与发烟硫酸反响来制取。将带有机械拌和装置的圆底烧瓶置于流水浴中,向其中参加560g100%的硫酸,在强烈拌和下将100g尿素分多次(约45min加完)渐渐参加到硫酸中,留意不要使温度超过40。然后向其中参加309g发烟硫酸(含65%游离SO3),并在42~45的温度下放置16h。用玻璃砂芯漏斗过滤反响混合物,先用纯硫酸洗刷,再用50%的硫酸洗刷,最后用冷的甲醇洗刷。
4. Aminosulfonic acid is the adduct of strong Lewis acid SO3 and strong Lewis base NH3. When preparing a few high purity amino sulfonic acid, it can directly react with ammonia with high purity SO3 under completely anhydrous conditions. If the dosage is large, the reaction between urea and fuming sulfuric acid can be used. Place the round bottom flask with mechanical mixing device in the running water bath. Participate 560 g 100% sulfuric acid in the flask. After strong mixing, add 100 g urea several times (about 45 minutes) and gradually participate in the sulfuric acid. Be careful not to make the temperature exceed 40. Then, 309g fuming sulfuric acid (containing 65% free SO3) was added and placed for 16 hours at 42-45 temperature. The reaction mixture is filtered by glass sand funnel. First, it is washed with pure sulfuric acid, then with 50% sulfuric acid, and finally with cold methanol.
5.将20%的发烟硫酸加热至30,渐渐参加尿素,温度控制在60~65,加完后保温3H,然后升温至80~85,保温2h,反响完毕后,冷却至5,过滤,所得结晶离心甩干后,用5%乙醇洗刷,滤干后用蒸馏水重结晶精制,得氨基磺酸纯品。
5. Heating 20% fuming sulfuric acid to 30, gradually participating in urea, temperature control at 60-65, heat preservation for 3H after adding, then heating to 80-85, heat preservation for 2h, cooling to 5 after reaction, filtering, crystallization centrifugal drying, washing with 5% ethanol, refining with distilled water after filtering, amino sulfonic acid pure product was obtained.
相关标签:氨基磺酸